阅读说明：本技术 一种利用核桃青皮色素染色羊毛纤维的染色方法 (Dyeing method for dyeing wool fibers by using walnut green husk pigment ) 是由 王雪梅 张文泰 易帆 郭潇涵 杨亮 陈莉萍 张天芸 于 2020-06-01 设计创作，主要内容包括：本发明公开了一种利用核桃青皮色素染色羊毛纤维的染色方法,属于纺织品印染技术领域。该染色方法包括步骤：将羊毛纤维调湿平衡后,在功率为560-700W的微波中预处理1-3min；利用核桃青皮色素染料原液对羊毛纤维进行染色,染色后进行水洗并自然晾干；染色的羊毛纤维浸入媒染固色液中,在功率为140-420W的微波条件下进行媒染固色,时间为1-5min；固色的羊毛纤维进行水洗并干燥后,即得核桃青皮色素染色的羊毛纤维。本发明通过利用核桃青皮色素进行浸染染色以及在功率为140-420W的微波条件下进行媒染固色,不仅降低了微波功率并缩短了固色时间,提高了固色效率并减少了微波能耗,而且染色后羊毛纤维的色差达到43.85,同时耐洗色牢度在4级以上。(The invention discloses a dyeing method for dyeing wool fibers by using walnut green husk pigment, belonging to the technical field of textile printing and dyeing. The dyeing method comprises the following steps: after the wool fibers are subjected to humidity adjustment and balance, pretreating for 1-3min in microwaves with the power of 560-700W; dyeing wool fibers by using walnut green husk pigment dye stock solution, washing with water after dyeing, and naturally drying; immersing the dyed wool fibers into a mordant color fixing solution, and carrying out mordant color fixing for 1-5min under the microwave condition with the power of 140-420W; and (5) washing and drying the fixed wool fibers to obtain the wool fibers dyed by the walnut green husk pigment. According to the invention, the walnut green husk pigment is used for dip dyeing and the mordant color fixation is carried out under the microwave condition of power of 140-.)

1. A dyeing method for dyeing wool fibers by using walnut green husk pigment is characterized by comprising the following steps:

the method comprises the following steps: after the wool fibers are subjected to humidity adjustment and balance, pretreating for 1-3min under the microwave condition with the power of 560-700W;

step two: dyeing wool fibers by using walnut green husk pigment dye stock solution, washing with water after dyeing, and naturally drying;

step three: immersing the dyed wool fibers into a mordant color fixing solution, and carrying out mordant color fixing for 1-5min under the microwave condition with the power of 140-420W;

step four: and (5) washing and drying the fixed wool fibers to obtain the wool fibers dyed by the walnut green husk pigment.

2. Dyeing process according to claim 1, characterized in that in step one the pretreatment is carried out under microwave conditions at a microwave power of 700W for a period of 3 min.

3. The dyeing method according to claim 1, characterized in that in said second step, wool fibers are dyed, comprising:

and dip-dyeing the wool fibers by using the walnut green husk pigment stock solution for 60min under the conditions of bath ratio of 1:50, pH of 4.5 and temperature of 80 ℃.

4. The dyeing method according to claim 1, characterized in that in the third step, the dyed wool fibers are fixed by mordant dyeing, further comprising:

carrying out mordant dyeing and color fixation on the dyed wool fiber under the conditions of bath ratio of 1:50, pH value of 4.5 and temperature of 80 ℃.

5. The dyeing method according to claim 4, wherein the mordant fixing solution is prepared from water, lanthanum chloride dissolved in the water and a reducing agent, wherein the dosage of the lanthanum chloride is 6-8% of the mass of the wool fibers, and the dosage of the reducing agent is 20-25 g/mL.

6. Dyeing process according to claim 1, characterized in that the fixing by mordanting under microwave conditions is carried out at a microwave power of 270W and a fixing time of 3 min.

7. Dyeing process according to claim 5, characterized in that the lanthanum chloride is used in an amount of 7% and the reducing agent in an amount of 22 g/mL.

8. The extraction method of the walnut green husk pigment stock solution is characterized by comprising the following steps:

the method comprises the following steps: dissolving walnut green husk powder by using 60v/v% ethanol solution, wherein the liquid-material ratio is 24:1 mL/g;

step two: extracting the dissolved walnut green husk powder under the microwave condition with the power of 450W for 1 min;

step three: standing the extractive solution to room temperature, filtering, and collecting ethanol pigment solution to obtain pigment stock solution of exocarpium Juglandis Immaturus.

Technical Field

The invention belongs to the technical field of textile printing and dyeing, and particularly relates to a dyeing method for dyeing wool fibers by using walnut green husk pigment.

Background

The walnut green husk is also called green dragon skin, is green epicarp of immature walnut, and has certain toxicity. As a main byproduct in the walnut industry, most of walnut green husks are directly discarded, the value is not fully developed and utilized, not only is the resource greatly wasted, but also the ecological environment is seriously polluted, and even the survival of animals and plants is threatened. In recent years, research on components and application of walnut green seedcase shows that the walnut green seedcase pigment is a safe and nontoxic natural pigment, has the characteristics of good water solubility, heat resistance and light resistance, easiness in biodegradation, no skin allergy or carcinogenicity, can be applied to printing and dyeing of silk, cotton and linen, leather, wool fabrics and the like, and has high application value in the dyeing industry. Therefore, the value of the walnut green husk pigment in printing and dyeing is researched, so that waste is changed into valuable, the economic benefit of fruit growers can be increased, and the comprehensive utilization value of walnuts is improved.

Wool is a natural protein fiber, and a hydrophobic scale layer structure exists on the surface of the wool, so that the adsorption and inward diffusion of dye are hindered, and the wool is difficult to dye, so that wool dyeing needs to be carried out at a higher temperature, and the dyeing time is longer. Although the dye-uptake can be improved by high-temperature dyeing, the wool fibers are damaged by long-time boiling dyeing, the problems of wool weight loss, rough hand feeling, yellow color, low spinning yield and the like occur, and the cost is increased.

Therefore, the exploration of low-temperature dyeing of wool is of great significance. Zhao Xue et al have discussed the microwave pretreatment and dyeing process of wool fabric, and disclose the dyeing process of wool fabric with active lanner element, including microwave pretreatment and dyeing process. Wherein, the microwave pretreatment is to dip the wool into urea solution and carry out microwave treatment with power of 700W for 5 min; the dyeing process flow comprises the steps of padding active dye solution → 700W power microwave heating color fixation for 6min → 40 ℃ water leaching → 80 ℃ ammonia water washing for 15min → 1 time water leaching → acetic acid neutralization; padding active dye liquor → rolling and stacking (20-0.5 ℃, 24 h) → washing with water; padding active dye solution → rolling and stacking for a certain time → microwave heating for color fixation for 6min → washing. The results show that: firstly, heating and fixing color of wool fabric by using microwave, wherein the apparent depth of wool deepens along with the increase of color fixing time; secondly, the wool fabric is dipped in water and urea solution, and the dye uptake of the wool fabric can be improved after microwave pretreatment; thirdly, the wool fabric has lower fixation rate but better uniformity in microwave heating fixation, and the leveling property is reduced after microwave pretreatment, but the microwave fixation and pretreatment can improve the dyeing fastness. However, this dyeing process has the following disadvantages: the method has the advantages that the microwave power is high, the heating time is relatively long, moisture of wool fibers is evaporated in a large amount in the color fixing process to be dried, the color fixing rate is influenced, even the fibers are damaged, the microwave energy consumption is high, the dyeing cost is increased, and the probability of microwave leakage is greatly improved.

Disclosure of Invention

In view of the above, the invention provides a dyeing method for dyeing wool fibers by using walnut green husk pigment, which not only reduces the microwave power in the dyeing process, but also shortens the color fixing time and improves the dye uptake and dyeing vividness.

In order to achieve the purpose, the invention adopts the following technical scheme:

the invention provides a dyeing method for dyeing wool fibers by using walnut green husk pigment, which comprises the following steps:

the method comprises the following steps: wetting and balancing the wool fibers under the common atmospheric condition, and then pretreating for 1-3min under the microwave condition with the power of 560-;

step two: carrying out dip dyeing on wool fibers by using walnut green husk pigment dye stock solution, washing with water after dyeing, and naturally drying;

step three: immersing the dyed wool fibers into a mordant color fixing solution, and carrying out mordant color fixing for 1-5min under the microwave condition of power of 140-420W;

step four: and (5) washing and drying the fixed wool fibers to obtain the wool fibers dyed by the walnut green husk pigment.

Preferably, in the first step, the microwave power for pretreatment under microwave condition is 700W, and the time is 3 min.

Preferably, in the second step, the wool fibers are dyed, including:

and dip-dyeing the wool fibers by using the walnut green husk pigment stock solution for 60min under the conditions of bath ratio of 1:50, pH of 4.5 and temperature of 80 ℃.

Preferably, in the third step, the mordant fixation is performed on the dyed wool fiber, and the method further comprises the following steps:

carrying out mordant dyeing and color fixation on the dyed wool fiber under the conditions of bath ratio of 1:50, pH value of 4.5 and temperature of 80 ℃.

More preferably, the mordant fixing solution is prepared from water, a mordant and a reducing agent dissolved in the water, wherein the mordant is lanthanum chloride, the dosage of the lanthanum chloride is 6-8% of the mass of the wool fibers, the reducing agent is sodium thiosulfate, and the dosage of the sodium thiosulfate is 20-25 g/mL.

More preferably, the microwave power for mordanting fixation under microwave condition is 270W, and the fixation time is 3 min.

More preferably, the dosage of the lanthanum chloride is 7 percent, and the dosage of the reducing agent is 22 g/mL.

The invention also provides an extraction method of the walnut green husk pigment stock solution, which comprises the following steps:

the method comprises the following steps: dissolving walnut green husk powder by using 60v/v% ethanol solution, wherein the liquid-material ratio is 24:1 mL/g;

step two: extracting the dissolved walnut green husk powder under the microwave condition with the power of 450W for 1 min;

step three: standing the extractive solution to room temperature, filtering, and collecting ethanol pigment solution to obtain pigment stock solution of exocarpium Juglandis Immaturus.

Compared with the prior art, the invention has the beneficial effects that:

according to the dyeing method provided by the invention, the walnut green husk pigment stock solution is used for dip dyeing and dye fixing, and mordant dyeing and color fixing are carried out under the condition that the microwave power is 140-;

the method utilizes lanthanum chloride as a mordant, so that the absorption wavelength of the walnut green husk pigment is increased, the dye uptake is improved, the color of the dyed wool fiber is deepened, the color brightness is also improved, the concentration of metal ions is reduced, the pollution of dyeing wastewater is reduced, and the method has the characteristics of environmental protection.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below.

FIG. 1 is a curve of the extraction rate of pigment from walnut green husk with the volume fraction of ethanol;

FIG. 2 is a curve showing the variation of the extraction rate of pigment from green husk of walnut with microwave power;

FIG. 3 is a curve showing the variation of the extraction rate of pigment from green husk of walnut with the extraction time;

FIG. 4 is a curve of the extraction rate of pigment from walnut green husk with the change of liquid-to-material ratio;

FIG. 5 is a plot of the shade difference of a mordant fixation sample versus fixation time;

FIG. 6 is a curve of the variation of the color difference value of a mordant fixation sample with the microwave power;

FIG. 7 is a plot of the variation of the color difference values of mordant fixation samples with the amount used;

FIG. 8 is a curve showing the variation of the color difference value of a mordant fixed color sample with the amount of a reducing agent;

FIG. 9 shows the surface morphology of a wool fiber without microwave treatment under a 40-fold electron microscope;

fig. 10 shows the surface morphology of microwave treated wool fibers under a 40-fold electron microscope.

Detailed Description

For the purpose of facilitating an understanding of the present invention, preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these descriptions are intended to further illustrate features and advantages of the present invention, and not to limit the claims of the present invention.